CN102356175A - Coatings, composition, and method related to non-spalling low density hardface coatings - Google Patents
Coatings, composition, and method related to non-spalling low density hardface coatings Download PDFInfo
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- 238000000034 method Methods 0.000 title claims description 17
- 238000000576 coating method Methods 0.000 title description 70
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- 238000005245 sintering Methods 0.000 claims description 52
- 239000000463 material Substances 0.000 claims description 43
- 239000003795 chemical substances by application Substances 0.000 claims description 28
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
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- 229910001000 nickel titanium Inorganic materials 0.000 description 1
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 description 1
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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- 229910052726 zirconium Inorganic materials 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12014—All metal or with adjacent metals having metal particles
- Y10T428/12028—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, etc.]
- Y10T428/12063—Nonparticulate metal component
- Y10T428/12097—Nonparticulate component encloses particles
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24802—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.]
- Y10T428/24893—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.] including particulate material
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Plasma & Fusion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Coating By Spraying Or Casting (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Powder Metallurgy (AREA)
- Laminated Bodies (AREA)
Abstract
A composite body that is spall resistant and comprises a substantially discontinuous cermet phase in a substantially continuous metal rich matrix phase. The composite body is typically bonded to a substrate to form a hardfacing on the substrate. The composite body exhibits ductile phase toughening with a strain to failure of at least about 2 percent, a modulus of elasticity of less than about 46 million pounds per square inch, and a density of less than about 7 grams per cubic centimeter. The metal rich matrix phase between the ceramic rich regions in the composite body has an average minimum span of about 0.5 to 8 microns to allow ductility in the composite body. The composite body has a Vicker's hardness number of greater than approximately 650.; The discontinuous cermet phase is in the form of ceramic rich regions embedded within the composite body, and it includes ceramic particles and a cermet binder. The ceramic particles having a Moh's hardness of at least approximately 7.5, a modulus of elasticity of less than approximately 46 million pounds per square inch, and an average particle size of from about 0.1 to 10 microns. The ceramic rich regions exhibit high hardness as compared with the matrix phase.
Description
Related application
The application requires to enjoy the rights and interests of No. the 61/149th, 680, the U.S. Provisional Application submitted on February 3rd, 2009.
The present invention is by government-funded; According to by at 1025F St; The contract #EPA EP-D-06-053 that the Bureau for Environmental Protection of Washington DC is authorized; Little composite coating of chromium quid pro quo; With according to by at Oklahoma City, the subcontract #USAF-0040-SC-0024-1 of the GDIT master contract #FA8601-04-F-0040 that the United States Air Force of OK is authorized carries out.
Background of invention
1. invention field.
The present invention relates generally to hard-surface coating, composition and method, and more specifically, embodiment of the present invention relates to and relevant hard-surface coating, composition and the method for anti-hard-surface coating that peel off, low-density.
2. description of the Prior Art.
The hard-surface coating especially coating based on chromium and tungsten that forms of the thermospray through composite powder is well-known, but they are easy to peel off usually, and they are heavy.For example, the tungsten-cobalt carbide coating of thermospray is stone, crisp and fine and close.Proposed through the thermospray pottery for example ceramic nitrides form coating, non-melt but pottery usually decomposes.For example, ceramic nitrides is decomposed down at about 1900 degrees centigrade.The thermospray operation is carried out in far away surpassing under 1900 degrees centigrade the temperature usually, and it is normally unsuccessful therefore to attempt to form coating through the thermospray ceramic nitrides.Previous the proposition used ceramic nitrides so that the coating that forms the control wearing and tearing and rub via physical vapor deposition and chemical vapor deposition operation, so but such vapour deposition tendency of operation slow with costliness.
It is the harder and coating that rigidity is stronger of cost manufacturing that the trial of past improvement wearing and tearing is usually directed to toughness.Generally speaking, because coating becomes harder and rigidity is stronger, the appearance of peeling off has increased.
The fusing of the material that the existing thermospray operation that is used to form hard-surface coating will be sprayed usually at least is as target, and usually also with the fusing of substrate surface as target.The thorough fusing of the powder that is sprayed is considered to useful and necessity usually, and this is because it has improved the chance that between coating and base material, forms the metallurgical binding that is different from mechanical bond.This thorough fusing makes the composition of coating become similar even fully usually.Existing typical thermospray is operated and is comprised, for example, and HVOF (high speed oxygen combustion gas), laser formation, plasma spraying, plasma transferred arc and analogue.
Regrettably; Because the coating of these thermosprays has high hardness; So the coating of these thermosprays is crisp, and during those situation that when receive the landing gear tube that impact, point loading or other heavily stressed situation for example use in ship-board aircraft in, exist, peeled off and bust.This peels off is to cause jointly through the stress in the increase high-modulus coating and the low strain tolerance level (strain tolerance) of high-modulus coating.In addition, these coatings are very fine and close, every cubic centimetre of about 8 gram for chromium carbide/nickel chromium triangle in the scope of every cubic centimetre of about 16 gram for the tungsten carbide/cobalt coating.The coating of these higher densities has increased sizable weight, has the low amount of passing through through the HVOF gun system, and makes the fuel combustion efficiency and the useful load of aircraft and other haulage system cause significant loss.At last, these have the extremely hard coating of limited flexible must be by superfinishing to prevent excessive sealing wear and the diamond of eliminating the surface spots cause initial failure.Because their fragility and high modulus, they on the surface with coating in flaw extremely responsive with defective, mean that they are very difficult to application, limited their effectiveness and the quantity of qualified applicator.
Outer space application examples such as the aircraft landing gear of heavily stressed and wearing and tearing need be on structural element hard-surface coating.Many such application had before related to the high-strength steel that uses WC-Co to coat.Proposed to replace such high-strength steel with titanium alloy, this is because can realize weight saving.The Young's modulus that titanium alloy has is less than the Young's modulus of previous high-strength steel.When previous WC-Co coating is crooked, have been found that peeling off of titanium appears in previous WC-Co coating.Need have low hard-surface coating to the Young's modulus that peels off that is enough to not occur titanium.For the purpose of weight reduction, proposed to have the structural member of thin cross section.Such structural member tends to bending and distortion.This causes peeling off of hard-surface coating.Need the toughness hard-surface coating again.The formation of toughness hard-surface coating before seemingly can not realize.It has been generally acknowledged that in same coating and can not obtain hardness and toughness.
Using thermospray to operate to form wherein isolating high ceramic content zone to be embedded into inhomogeneous coating in the toughness substrate is disclosed in No. the 2007/0141270th, the U. S. application of announcement of the Sherman that announced on June 21st, 2007; This U. S. application is incorporated this paper in view of the above by reference into, as setting forth fully at this.
The people that pay close attention to these problems recognize the demand to improved hard-surface coating.
The invention summary
The present invention is in response to the current state of this area and especially develop with other problems and demand in response to these that also fully or fully do not solve through current available way.Therefore, catalogue of the present invention is to solve problem and the shortcoming that this paper confirms effectively at least.Embodiment of the present invention is suitable as especially that soundness, reliability, weather resistance and low density are the hardened faces (hardfacing) of the outer space structural element of important factor for functional and security.
Embodiment of the present invention comprises the heterogeneous composite material main body, and this heterogeneous composite material main body is anti-that peel off and comprise the discontinuous basically sintering metal phase during the rich metal matrix of successive basically mutually.
Do not need base material although can independently work, in some embodiments, composite body is incorporated into base material, for example, such as steel, titanium, aluminium or their alloy, their high-strength alloy especially.Such base material is normally for the purpose of wear-resistant, soundness, corrosion-resistant and weather resistance and need the metal of hardened face.
Composite body demonstrates with at least about the toughness phase of 2% breaking strain malleableize, less than the Young's modulus of about 0.46 hundred million pound per square inch; In some embodiments less than about 7 density that restrain every cubic centimetre; And in other embodiment, less than the density of every cubic centimetre of about 6 gram.Rich metal matrix between the rich ceramic region in composite body has about 0.5 to 10 micron average span mutually to allow the toughness of composite body.Composite body has the vickers hardness number (VHN) greater than about 650 in some embodiments, and in other embodiment, has greater than about 750 the VHN up to about 1200.
Discontinuous sintering metal is the form that is embedded in the rich ceramic region in the composite body mutually, and comprises ceramic particle and sintering metal tackiness agent.Ceramic particle has the Mohs' hardness at least about 7.5; And in some embodiments; Have Mohs' hardness from about 8 or 9, less than the Young's modulus of about 0.46 hundred million pound per square inch; And have in some embodiments, less than the Young's modulus of about 0.40 hundred million pound per square inch with from about 0.1 to 10 micron mean particle size.Than matrix phase, rich ceramic region demonstrates high hardness.
According to some embodiment, the heterogeneous composite material main body is through preparing fine ceramics particle and abundant dispersive sintering metal tackiness agent agglomeration in the core metal ceramic particle.Then core metal ceramic particle and rich metal matrix are formed combination of materials and become composite body.Combination operation can be carried out through the thermospray operation of routine, conventional electrodeposition process or similar operations.When adopting thermospray to form composite body, core metal ceramic particle and rich metal matrix are formed combination of materials, become the raw material that is used for the thermospray operation.Thermospray operation can be for example carried out according to the instruction of announcing No. the 2007/0141270th, U. S. application of Sherman.Have been found that the HVOF hot-spraying techniques is particularly suitable for the production of some embodiment of the present invention.When adopting conventional electrolyting precipitation process, the core metal ceramic particle can only be dispersed in the bath, makes them when coating forms, be captured in the coating.
For the technician who makes the relevant field that is closely related most with the present invention knows, the accompanying drawing of the part of this paper through forming specification sheets and describing has with reference to the accompanying drawings been illustrated the embodiment of composite body of best mode that is used for the present invention is dropped into the present expection of practice.Describe exemplary embodiment in detail, and do not attempt to illustrate all various forms and the modification that the present invention possibly comprise.Therefore; The shown embodiment with description of this paper is illustrative; And as will become tangible for those skilled in the art; Can in scope of the present invention and spirit, make amendment in many ways, the present invention delimits by appended claim rather than by the details of specification sheets or accompanying drawing.
The accompanying drawing summary
The present invention provides its benefit in multiple stiff dough is used, stiff dough is used and comprised outer space, mining, oil and gas-field exploitation and exploitation, equipment repair, farming and preparation of construction and analogue.Although the many such application of the description of hereinafter following intention representative, it is not an exhaustive.To be familiar with like those skilled in the art, base composition, composite body and the method for this paper instruction can easily be suitable for many purposes.This specification sheets should meet and scope of the present invention that is disclosed and the consistent width of spirit with the claim that invests this, although some possibly seem the restricted language of forcing by about the needs of disclosed specific examples.
Only in order to illustrate the purpose of the present invention and its best mode understood at present rather than restriction, especially with reference to the accompanying drawings:
Fig. 1 has described to be used to produce the schema according to an embodiment of heterogeneous composite material main body of the present invention.
Fig. 2 has described the embodiment according to agglomerant core metal ceramic particle of the present invention with graphics.
Fig. 3 has described the embodiment according to the cermet particles of the coating that is suitable as the raw material in the thermospray operation of the present invention with graphics.
Fig. 4 has described to form according to the matrix of core metal ceramic particle that is suitable as the raw material in the thermospray operation of the present invention and joint the other embodiment of rich metallic particles with graphics.
Fig. 5 has described the implementation of processes mode according to formation heterogeneous composite material main body of the present invention with graphics.
Detailed description of the preferred embodiment
With reference now to accompanying drawing,, wherein in whole some secondary views, identical reference number refers to identical or corresponding parts.Should be understood that accompanying drawing is the illustrated of various embodiments of the present invention and schematic expression, and be interpreted as limiting the present invention never in any form.This paper is not intended to the meaning of such speech and phrase is limited to those concrete embodiments about the speech of concrete embodiment and the use of phrase.Only if this paper at length sets forth concrete definition, otherwise the speech of this paper and phrase intention have their common meanings in this area.
Specifically with reference to the accompanying drawings, in the embodiment of selecting for the purpose of illustrating, illustrate the core metal ceramic particle of forming by the agglomerant intimate mixture of ceramic particle and sintering metal tackiness agent with 10 usually.In the embodiment of Fig. 3, the core metal ceramic particle is encapsulated in the continuous coating basically 12 of rich metal matrix formation material.In the embodiment of Fig. 4, the particle 14 that typical rich metal matrix forms material links with core metal ceramic particle 10 through being attached to the core metal ceramic particle in the discontinuous coating.
In the embodiment of Fig. 5; Composite body 16 is through with the formation of getting off: select agglomerant and fixed core metal ceramic particle 18; In encapsulation steps 26, it is coated, to form the cermet particles that is coated continuously basically 20 that is encapsulated in basically in the rich metal matrix formation material 28.The cermet particles 20 that is coated is supplied as the raw material of thermospray step 32.The cermet particles 20 that remollescent is coated is collided on the base material (not shown) to form composite body 16.Basically cermet particles 20 distortion that coated continuously are to form the discontinuous sintering metal phase in the composite body 16.At the embodiment of selecting to be used for illustrating; Discontinuous sintering metal comprises rich ceramic region 34 mutually, and rich ceramic region 34 is usually and is embedded in the rich metal matrix of successive basically mutually in 36 and usually by the sedimental form of 36 lens shapes that are spaced apart from each other mutually of the rich metal matrix of successive basically.Rich ceramic region 34 is formed by the core metal ceramic particles 18 of distortion usually, and rich metal matrix phase 36 forms material 28 by rich metal matrix usually and forms.Additive 30 can be included in any stage that forms cermet particles.Such additive is usually with 30 indications.Such additive is normally conventional, and comprises them for performance or the character that advantageously changes cermet particles.Rich ceramic region is usually by spaced apart like common spans with 38 and 40 indications.The shape and size of span are irregular, but demonstrate the mean distance of the ratio control of the cermet particles 20 that mainly forms material 28 by rich metal matrix and coated.Span is filled up the rich metal matrix phase 36 of successive basically.Like what illustrate among Fig. 4, the cermet particles 20 that replaces successive basically to be coated with the discontinuous cermet particles that is coated provides substantially the same composite body 16.The particle (not illustrating) that uses loose rich metal matrix to form material produces substantially the same composite body 16, and condition is that raw material is mixed so that form loose discontinuous coating around the core metal ceramic particle cmpletely.
According to some embodiment, composite body has the breaking strain greater than 1%, and in some embodiments, has about breaking strain of 2% to 6% and from about 0.46 to 0.20 or the modulus of 0.40 to 0.25 hundred million pound per square inch.In some embodiments; Rich metal matrix has about 0.5 to the 10 micron average span between the sintering metal zone of discontinuous sintering metal phase mutually; And in some other embodiments, has about 0.4 or 0.5 minimum span; Up to about 8 microns maximum span, and in some other embodiments, have from about 0.5 to 2 micron span.
The span that has been found that the metal matrix phase between the sintering metal zone has caused the toughness of composite body basically.The span of rich metal matrix is the character with toughness phase inclusion of minimum average B configuration size.Span must be enough to allow the work hardening of rich metal matrix phase.Have been found that about 0.4 to 0.5 micron minimum span is that the acquisition appropriate toughness is needed.If this span is too little, then exist seldom or do not have work hardening, and composite body tends to break when being subjected to stress.If average span greater than the average span that allows work hardening to need (usually less than about 8, and about in some embodiments 6 or 52 or littler micron), then the hardness of composite body, density and wear resistance possibly be not enough to the purposes that is used to expect.For specific sintering metal-Fu metal-matrix composite, the sintering metal in the composite body is proportional with rich metal matrix amount mutually, to obtain best average span.For some embodiment, the approximation (use rule of mixture) of best ratio through initial calculation is that the iterative process of actual test is confirmed subsequently.
Rich metal matrix comprises tough metal mutually.Rich metal matrix extends between the rich ceramic region that is formed by cermet particles.Some embodiment for example utilizes at least a as tough metal in following: nickel and cobalt and their alloy; Ni-Ni
3P, NiP, Ni
2P; Ni-Cr; Fe-Cr-Al; Ni-Ni
2B, Co-Co
3The mixture and the alloy of P, Fe-Al alloy, Ni-Al alloy, titanium and its alloy (comprising the Ni-Ti alloy), copper and its alloy and these materials.The corresponding modulus that has less than about 0.42 hundred million pound per square inch of rich metal matrix, and have modulus in some embodiments less than about 0.35 hundred million pound per square inch.The modulus that is demonstrated by chromium is 0.42 hundred million pound per square inch.The metal of rich metal matrix in mutually should be in about 1900 degrees centigrade (decomposition temperatures of silicon nitride) fusing down.React significantly with pottery under the temperature that the material of rich metal matrix in mutually can not run in the thermospray operation.
Rich metal matrix form material constitute usually the raw material that forms composite body from about 5 to 30V%, and according to some embodiments, from about 5V% or 10V% or 15V% to 20V% or 25V% or 30V%.Cermet particles as the raw material in the thermospray operation is in 10 to 60 microns mean particle size usually, and from 20 to 50 microns mean particle size in some embodiments.The sintering metal granularity depends primarily on the requirement of employed particular spray gun, and the thermal mass of particular particles and density.Generally speaking, tend to stop up many spray guns in the granularity below 10 microns, and tend to cause the base material that is sprayed to carry out sandblasting at the particle more than 60 microns.
According to some embodiment, composite body has the density less than every cubic centimetre of about 6 gram.In order to obtain this density, when still obtaining required breaking strain and modulus properties simultaneously, must make the amount of low-density ceramic maximum.When mode of administration relates to thermospray, and relate to ceramic nitrides, then have other consideration item.Between sintering metal tackiness agent and ceramic nitrides, there is balance.Ceramic nitrides is decomposed rather than fusing usually.For example, Si
3N
4Decompose down at about 1900 degrees centigrade.Thermal spray system is operated being significantly higher than under the temperature of this decomposition temperature usually.Decompose under the temperature that unshielded nitride ceramics adopts in the thermospray operation usually.When the sintering metal tackiness agent is distributed in the sintering metal (for example, through the coating ceramic particle, or employing and mean diameter are the mixing time of the prolongation of about one micron sintering metal adhesive particle) cmpletely, the decomposition of less generation ceramic particle.Although do not hope to be subjected to any theory, fully the sintering metal tackiness agent that distributes tends to keep gaseous decomposition product closely to contact with ceramic particle significantly, so decomposition reaction is downtrod on kinetics.This needs enough sintering metal tackiness agents and sintering metal tackiness agent enough to be distributed fully to suppress the decomposition of ceramic particle.According to some embodiments, during thermospray, decompose less than about 20% ceramic nitrides.If there are not enough sintering metal tackiness agents that distributes fully in the sintering metal, then rate of decomposition is near 100%.For some embodiment, for the combination of specific ceramic-metal ceramic binder, best ratio and the married operation approximation (based on rule of mixture) through initial calculation is that the iterative process of actual test is confirmed subsequently.According to some embodiment, ceramic particle constitute agglomerant core metal ceramic particle from about 30 to 80 or from about 40 to 70 or from about 40 to 50 volume %.
According to some embodiment, the mean particle size of ceramic particle is about 0.01 or lower in about 10 microns scope.In other embodiment, the ceramic particle mean particle size in the scope of about 0.1 to 8 micron or 0.3 to 8 micron, and in other embodiment in about 0.3 to 5 micron scope.For greater than about 8 to 10 microns average ceramic granularity, resulting composite body is tended to demonstrate than by having corrosion rate and high corrosion rate and the wear rate of wear rate that the composite body of size at about ceramic particle below 10 microns demonstrates.The actual lower limit of pottery granularity is processed limitation and is retrained.About ceramic granularity below 0.1 micron becomes and is difficult to produce consistent even metal pottery.
According to some embodiment, ceramic particle is the pottery with high hardness ratio.That is, such pottery has high hardness and low modulus.Suitable pottery with essential hardness and low Young's modulus comprises, for example the nitride of silicon, titanium, chromium, vanadium, aluminium, zirconium, niobium, carbonitride and oxynitride with and composition thereof, zircon, zirconium white, sapphire and mullite.Aluminum oxide has the modulus of about 0.48 to 0.50 hundred million pound per square inch individually, but its can be satisfactorily with have than other ceramic blend of low modulus or its and can be used with low volume fraction.Zircon has the modulus of about 0.21 hundred million pound per square inch, and zirconium white has the modulus of about 0.35 hundred million pound per square inch.Mullite has about 9 the Mohs' hardness and the modulus of about 0.38 hundred million pound per square inch.In some embodiments, ceramic particle comprises at least a in the following material: Si
3N
4, TiN, VN, V
2N, CrN, Cr
2N, ZrN, Nb
2N, TiCN, SiCN, SiON or SiAlON.Nitride demonstrates low friction and high and thermal compatibility metal usually.
In some embodiments, the sintering metal tackiness agent comprises having less than about 5 microns metallic particles up to about 0.5 micron mean particle size, and in other embodiment, comprises the metallic particles that has from about 2 to 0.5 microns mean particle size.For the purpose of security, the granularity of the sintering metal tackiness agent of metal should be in that they become more than the granularity of explosive substance when being exposed to air.According to some embodiment, suitable metal comprises, the alloy of Ni, Co, Fe and they and Cr, Al and Ti for example, with and composition thereof.In other embodiment, the sintering metal tackiness agent is the metallic coating on ceramic particle.Such metallic coating is used through routine techniques, and routine techniques comprises for example chemical vapour deposition, is coated onto at metal and acutely mixes under the condition on the pottery or mill or similar techniques.
For the existing hard-surface coating especially hard-surface coating on heavily stressed and lamellar structure parts, peeling off becomes serious problem.Peeling off is the combination of modulus (for given amount of deflection, the amount of cumulative stress) and toughness or strain tolerance level.This is not only a modulus, but with the staggered modulus of adhesion strength and the combination of toughness or toughness.Pottery has the strain tolerance level less than 0.7% usually, and has high modulus and common poor adhesivity concurrently.Previous hardened face material has the strain tolerance level toughness (WC-Co is about 0.5-0.8%) of high modulus, relative mistake usually.Composite body according to the present invention has low modulus; Or the base material that is attached to it has very low modulus mismatch (when steel is used as base material; In ideal conditions with the steel coupling); So have very low strain mismatch, good adhesion (about 10; More than 000 pound per square inch) and very high toughness or strain tolerance level (more than 1%; And in most of embodiment about more than 2%, and for some embodiments about more than 3%).The strain tolerance level means and deviates from work hardening and strain is re-oriented into away from the distorted area, and this is not the character of being enjoyed by existing hard-surface coating usually.The following instance of the optimal mode of at present contemplated embodiment of the present invention will be explained practice of the present invention and made those skilled in the art expect other embodiment.
Embodiment 1
Agglomerant little composite powder is through the Si of 0.5 micron of ball milling in ball mill
3N
4The Ni of powder and 40 weight % (wt%) and the Cr powder of 10wt% reach 24 hours and prepare.This instance is illustrated in Fig. 1 with graphics.Add poly (vinyl alcohol) binder together with water and conventional tensio-active agent so that the viscosity of resulting slurry drop between 200 and 300 centipoises.Agglomerant powder forms through the spraying drying slurry.Use centrifugal atomizer to come the spraying drying slurry, to produce about spheric, free-pouring agglomerant powder with 15,000 rpms, 300 degrees centigrade the gas temperature and the temperature out of 180 Fahrenheit degrees.These powder are taken off constraint down at 200 to 300 degrees centigrade in hydrogen, and under 1250 degrees centigrade, are sintered 2 hours to produce fine and close, free-pouring powder, and wherein about half particle has about 38 microns diameter.The screening powder with produce-270 ,+400 orders hold back (mesh cut).In fluidized-bed reactor, adopt the decomposition of nickle carbonoxide to come further to coat the powder that sieved with 10wt% nickel.Use then utilize liquid kerosene to act as a fuel and agglomerant powder spraying that oxygen coats nickel as the TAFA JP8000 thermal spray system (being made by Tafa Division of Praxair) of oxidant gas to the M300 steel substrate of sandblasting.Resulting coating has about 720 vickers hardness number (VHN), greater than the adhesion strength (combining the pin adherence tests) of about 10,000 pound per square inch gages according to ASTM 622.Coating has less than 180 about 0.5 inch degree bending radius and about 5.6 density that restrain every cubic centimetre.When confirming bending radius, sample is become " U " shape around the bent spindle of 1/2 inch diameter, and do not make coating cracking or break.This coating holds out against the 180KSI Fatigue Test when R=-1.0, and does not have sign cracked or that peel off.Fatigue Test carries out 4140 (M300) steel that is coated and uses ASTM E 466 to measure.This steel that is not coated has 220KSI safe range of stress value.Through comparing, the WC-Co coating is peeled off at about 160KSI usually.Young's modulus uses rule of mixture to calculate, and is about 0.35 hundred million pound per square inch.The breaking strain of coating is estimated from the bending radius in when cracking, is about 4%.When repairing aircraft actuator and landing gear tube, this coating is suitable for replacing chromium and WC-Co hardened face.Embodiment according to the coating of this examples preparation will demonstrate usually about 5; 000 pound per square inch gage (psig) compressive residual stress and about 3; Unrelieved stress between the 000psig stretching unrelieved stress; And in other embodiment; In approximate adiaphorous stretching unrelieved stress to about 2, between the 000psig compressive residual stress.Repeat this instance and will produce following coating: when 4340 or the 300M steel on have about 5 to 7 mils thickness the time will under fully reverse (R=-1) load of about 210KSI, withstand at about 200KSI at least about 200 circulations.When being applied to the steel of other known superstrengths, the embodiment of such coating will provide similar result.
Embodiment 2
The titanium nitride powder (being made by Kennametal inc) that in Segvari type masher, will have about 1 to 3 micron mean particle size mechanically fused 24 hours with 32wt%Ni and 8wt%Cr powder (about 1 to 5 micron mean particle size).Masher is made by Union Process.All powder are-325 orders.Will be mechanically the interfused powder from grinding machine shift out, drying, use high-shear mixer then and use NH
3Water-2% polyvinyl alcohol solution the blend of OH alkalization is with the slurry of the solids content that produces about 45 volume % (V%), and this slurry has the viscosity between 100 to 300 centipoises.Slurry is sprayed to produce the agglomerant powder of about 34 microns mean particle sizes with 18,000 rpms through FU11 centrifugal atomizer (making) by NIRO.Spray-dired agglomerating powder is taken off constraint under about 200 to 300 degrees centigrade in hydrogen.When the agglomerated particle that is taken off constraint is sintered about 3 hours when producing fine and close fully basically little composite core sintering metal under about 1200 degrees centigrade, the agglomerated particle that is taken off constraint keeps their size basically.Also in fluidized-bed, in the presence of oxygen, adopting the decomposition of nickel salt (etheric acid nickel monohydrate) to come under 350 degrees centigrade with the agglomerant core material of 10wt% nickel metallic cover.Then little composite powder is sprayed on the 4340M high-strength steel base material that is cleaned with sandblasting.The condition of thermospray is to make TiN partly decompose, and produces the TiN through the rich Ti of the modulus calculated with 0.42 hundred million pound per square inch (295Gpa).Coating has the microhardness of 838VHN; The sour environment of seeing in the acid resistance oil extremely; Has breaking strain greater than about estimation of 3 to 4% (based on cracking time bending radius); Have and surpass 10; The density that the sticking power of 000 pound per square inch gage (ASTM 622) and about 6.3 grams are every cubic centimetre.Young's modulus calculates from rule of mixture, is about 0.41 hundred million pound per square inch.The coating that should be suitable for the gun drilling parts based on the coating of TiN comprises that experience is corroded and rod, bearing, pump shaft, sealing member, rotor and the valve body of eating condition.
Embodiment 3
Preparation 0.3-0.8 micron α SiAlON powder is (at Al
2O
3And Si
3N
4Between about 1.2 modes) and with itself and the blend of 40V%Ni-Cr tackiness agent.This blend is sprayed dry also sintering to form the agglomerant slug particle of about 35 micron diameters.This particle passes through conventional electroless plating subsequently with 5 Ni-Ni that arrive 7V%
3The P nano composite material coats.These powder use high speed oxygen combustion gas (HVOF) thermal spray system to spray then, to produce fine and close fully basically coating, this coating demonstrates 800 to 950VHN hardness and the bend ductilitys between 3 and 5%, as using ASM bend ductility sample measurement.1/32 inch thick 6 inches long steel plate is by the coating (2 to 3 mil) of thermospray to form 50 to 70 micron thick.With this sample is the tapering spindle bending of 0.5 to 1 inch diameter change around diameter.Bend ductility is observed estimation then first from cracking or striped.1 inch is bent into about 3.5% toughness, and 0.5 inch bending diameter is about 7% toughness.Demonstrate cracking during at about 0.75 inch bending diameter in the coating on this sample.Young's modulus is estimated from rule of mixture, is about 0.37 hundred million pound per square inch.Breaking strain is estimated from the bending radius in when cracking, is about 4.5%.This coating can use belt sanding or other fast and cheaply finishing technology come precision work.At the WC-Co that does not need very high hardness (or cost), but in need the application than high wearability of the wearability that can be provided by hard chrome and erosion resistance and erosion resistance, these coatings be suitable as the quid pro quo of WC-Co.
Before, it was suggested that various additives and properties-correcting agent were used to form and use the various purposes of different metal ceramic product.Such additive comprises, for example wetting agent, grain growth inhibitor, fusing point conditioning agent and analogue.Optional properties-correcting agent and additive are comprised in the cermet particles with 30 indications (Fig. 5).Properties-correcting agent and additive are commonly used to promotion and adhere to, or limit grain growth, or restriction diffusion or reaction, or otherwise change temperature of fusion, physical properties, mechanical properties or chemical property or similar.
Especially when adopting thermospray to form composite body, all material of participating in composite body is comprised in the metal ceramic powder.Therefore, the composition of composite body and physical configuration are at least mainly by confirming together with the condition that forms main body forming with configuration of cermet particles.
The sintering metal tackiness agent can comprise change sintering metal tackiness agent and/or the physical properties of composite body or the enhancing inclusion or the dissolved material of chemical property.Generally speaking, the sintering metal tackiness agent is the tough metal greater than 50 volume %.
The metal matrix presoma that forms the rich metal of the rich metal matrix phase in the composite body comprises greater than half and in some embodiments greater than the tough metal of about 75 volume % usually.Rich metal matrix persursor material can comprise the enhancing inclusion or the dissolved material of the physical properties or the chemical property of the rich metal matrix phase that changes composite body.
According to composite body of the present invention original position formation on substrate surface usually.That is, than forming, be transferred in other place and being administered to substrate surface, composite body is formed by cardinal principle fluid state original place.Form by approximate fluid state original position and to make main body as far as possible closely be attached to base material.When combining is mechanical, and the composite body that original position forms meets stayed surface with the mode that can not realize with the main body that forms separately on minor detail.Original position forms and makes main body meet arcuate surfaces or angle surface is arranged, or has had a mind to provide the surface of anchoring configuration or roughness.
Composite body is formed on smooth, the arciform of base material expediently or has on the surface at angle.Base material has the physical features of the physical features that is different from composite body usually.Usually, the substrate support composite body also provides intensity to composite body, and main body is that base material provides wearability and hardness.When composite body intention was separated with base material, base material can be to remove and do not damage low melting point alloy or the material or the analogue of composite body through leaching.When the needs metallurgical binding, the surface of base material can coat with adhesionpromoter in advance.Adhesionpromoter comprises, for example, forms aluminium or other elements of low melting point alloy with rich metal matrix.In the time will forming mechanical bond, the mating surface of base material can be coarse or porous.
The rich metal matrix that engages with cermet particles presoma mutually can for example be following form: metallic coating, particulate substantially loose adherent settling, be in loose but the particle or the analogue of intimate admixture relation with ceramic particle.In some embodiments, the tough metal content in the rich metal matrix phase presoma is higher than the metal content in the metal ceramic powder.
Metal deposit can be formed on ceramic particle and the sintering metal slug particle, like what can expect through machinery, chemistry, electrochemical, vapour deposition, agglomeration, sintering or other conventional settling forming processes.If necessary, can adopt that purpose for the integrity of improving cermet particles or its component or other character for example cleans, activation, precoating or the various treatment steps that similarly carry out.Rich metal matrix phase presoma can be formed in one or several operate continuouslys on the sintering metal slug particle, with at identical or such persursor materials that the various conditions deposit is identical or different.
What described is preferred embodiment, wherein can make amendment and change, and do not depart from the spirit and scope of appended claim.According to instruction above, many modifications of the present invention and version are possible.It is therefore to be understood that in the scope of appended claim the present invention can be different from like concrete described the practice.
Claims (22)
1. composite body; Said composite body is anti-that peel off and comprise the discontinuous sintering metal phase during rich metal matrix mutually; Said discontinuous sintering metal comprises ceramic particle and sintering metal tackiness agent mutually; Said ceramic particle has Mohs' hardness at least about 8, less than the modulus of about 0.46 hundred million pound per square inch with from about 0.1 to 10 micron mean particle size, said composite body has vickers hardness number greater than about 650, at least 1% breaking strain and less than the modulus of about 0.46 hundred million pound per square inch.
2. composite body as claimed in claim 1, wherein said composite body is incorporated into base material.
3. composite body as claimed in claim 1, wherein said composite body have from about breaking strain of 2% to 6%.
4. composite body as claimed in claim 1, wherein said composite body have from about 46,000,000 to 20,000, the modulus of 000 pound per square inch.
5. composite body as claimed in claim 1, wherein said sintering metal tackiness agent comprises metal.
6. composite body as claimed in claim 1, wherein said rich metal matrix comprise nickel, iron, copper, cobalt, silicon, itself and at least a in the alloy of alternative alloy or itself and chromium, tungsten or molybdenum in them mutually.
7. composite body as claimed in claim 1, wherein said composite body have the density less than every cubic centimetre of about 6 gram.
8. composite body as claimed in claim 1, wherein said ceramic particle have less than about modulus of 46,000,000 with at least about 8 Mohs' scale hardness.
9. composite body as claimed in claim 1, wherein said ceramic particle comprise at least a in nitride, oxynitride or the carbonitride.
10. composite body as claimed in claim 1, wherein said ceramic particle comprises Si
3N
4, TiN, VN, V
2N, CrN, Cr
2N, ZrN, Nb
2At least a among N, TiCN, SiCN, SiON or the SiALON.
11. composite body as claimed in claim 1, wherein said ceramic particle comprises SiAlON.
12. composite body as claimed in claim 1, wherein said rich metal matrix has about 0.5 to 10 micron average span mutually.
13. composite body as claimed in claim 1, wherein said rich metal matrix has about 0.5 to 2 micron average span mutually.
14. composite body as claimed in claim 1, wherein said discontinuous sintering metal generally include the island that embeds a plurality of lens shapes that approximately extend in parallel of said rich metal matrix in mutually mutually.
15. composite body as claimed in claim 1, wherein said ceramic particle have from about 0.3 to 8 micron mean particle size.
16. composite body; Said composite body is anti-that peel off and comprise the discontinuous sintering metal phase during rich metal matrix mutually; Said discontinuous sintering metal comprises ceramic particle and sintering metal tackiness agent mutually; Said ceramic particle has the Mohs' hardness at least about 8; Less than about 46; 000; The modulus of 000 pound per square inch and from about 0.1 to 10 micron mean particle size; Said composite body has the vickers hardness number greater than about 650; Breaking strain at least about 2%; Less than the density of every cubic centimetre of about 7 gram with less than the modulus of about 0.46 hundred million pound per square inch, and said rich metal matrix has from about 0.4 to 10 micron average span mutually.
17. composite body; Said composite body is anti-that peel off and comprise the discontinuous sintering metal phase during rich metal matrix mutually; Said discontinuous sintering metal comprises ceramic particle and sintering metal tackiness agent mutually; Said ceramic particle has the Mohs' hardness at least about 8; Less than about 46; 000; The modulus of 000 pound per square inch and from about 0.3 to 8 micron mean particle size; Said composite body has the vickers hardness number greater than about 750; From at least about 2% to about 6% breaking strain; Less than the density of every cubic centimetre of about 6 gram with less than the modulus of about 0.46 hundred million pound per square inch, and said rich metal matrix has about 0.5 to 2 micron average span mutually.
18. composite body; Said composite body is anti-that peel off and comprise the discontinuous sintering metal phase during rich metal matrix mutually; Said discontinuous sintering metal comprises ceramic particle and sintering metal tackiness agent mutually, and said composite body has vickers hardness number greater than about 650, the breaking strain at least about 2% and less than the modulus of about 0.46 hundred million pound per square inch.
19. composite body as claimed in claim 18, wherein said composite body adheres to metal base with the adhesion strength greater than about 10,000 pound per square inch gages.
20. composite body as claimed in claim 18, wherein said ceramic particle has the modulus less than about 0.4 hundred million pound per square inches.
21. a method that on base material, forms composite body comprises:
Select cermet particles; Said cermet particles comprises sintering metal slug particle, sintering metal tackiness agent and the rich metal matrix presoma mutually that contains ceramic particle; Said rich metal matrix phase presoma comprises from the said cermet particles of about 20 to 70 volume %; Said ceramic particle has Mohs' hardness at least about 8, less than about 46; The modulus of 000,000 pound per square inch and from about 0.3 to 8 micron mean particle size;
Said cermet particles is injected in the thermal spray generation device;
Make said thermal spray generation device produce the thermal spray that comprises said cermet particles;
Said thermal spray is directed on the base material; With
Allow said composite body on said base material, to form.
22. a method for preparing cermet particles, said cermet particles are applicable to through thermospray the composite body of high rigidity low modulus is applied to base material, said method comprises:
Selection has Mohs' hardness at least about 8, less than the modulus of about 46,000,000 pound per square inch with from the ceramic particle of about 0.01 to 10 micron mean particle size,
Selection has the sintering metal tackiness agent less than about 5 microns mean particle size;
Said ceramic particle of intimate admixture and agglomeration and said sintering metal tackiness agent are to form even metal ceramic core particle basically, and wherein said ceramic particle comprises the agglomerant core metal ceramic particle from about 30 to 80 volume %;
Closely combine said sintering metal slug particle with from the rich metal matrix of about 5 to 30 volume % mutually presoma to form said cermet particles; With
Reclaim said cermet particles.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US14968009P | 2009-02-03 | 2009-02-03 | |
| US61/149,680 | 2009-02-03 | ||
| PCT/US2010/023097 WO2010123612A2 (en) | 2009-02-03 | 2010-02-03 | Coatings, composition, and method related to non-spalling low density hardface coatings |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102356175A true CN102356175A (en) | 2012-02-15 |
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ID=42540638
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010800122672A Pending CN102356175A (en) | 2009-02-03 | 2010-02-03 | Coatings, composition, and method related to non-spalling low density hardface coatings |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US8460796B2 (en) |
| EP (1) | EP2393954A2 (en) |
| CN (1) | CN102356175A (en) |
| BR (1) | BRPI1005423A2 (en) |
| CA (1) | CA2751250C (en) |
| SG (1) | SG173515A1 (en) |
| WO (1) | WO2010123612A2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109177367A (en) * | 2018-09-07 | 2019-01-11 | 昆明理工大学 | A kind of discontinuous stratiform structural composite material and preparation method thereof |
| CN109844177A (en) * | 2016-08-16 | 2019-06-04 | 塞拉姆涂料股份有限公司 | The thermal spraying of ceramic material |
| CN111148567A (en) * | 2017-10-13 | 2020-05-12 | Sabic环球技术有限责任公司 | Process for producing an elastomer agglomerate composition, elastomer agglomerate composition and use thereof |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9376573B2 (en) * | 2009-02-03 | 2016-06-28 | Mesocoat Inc. | Coatings, composition and method related to non-spalling low density hardface coatings |
| MY167015A (en) | 2011-03-10 | 2018-07-31 | Mesocoat Inc | Method and apparatus for forming clad metal products |
| US20140234549A1 (en) * | 2013-02-15 | 2014-08-21 | Mahle International Gmbh | Thermally sprayed wear-resistant piston ring coating |
| EA201591818A1 (en) | 2013-03-15 | 2016-07-29 | Месокоут, Инк. | THREE-COMPONENT CERAMIC POWDER FOR THERMAL SPRAY APPLICATION AND METHOD OF COATING THERMAL SPRAY |
| US9611532B2 (en) * | 2013-07-03 | 2017-04-04 | Mahle International Gmbh | Coating additive |
| US9943918B2 (en) * | 2014-05-16 | 2018-04-17 | Powdermet, Inc. | Heterogeneous composite bodies with isolated cermet regions formed by high temperature, rapid consolidation |
| US10538871B2 (en) | 2016-11-24 | 2020-01-21 | Samsung Electronics Co., Ltd. | Washing machine |
| CA3002295A1 (en) * | 2017-06-21 | 2018-12-21 | Rolls-Royce Corporation | Impurity barrier layer for ceramic matrix composite substrate |
| US11976013B2 (en) | 2017-09-27 | 2024-05-07 | Rolls-Royce Corporation | Composite coating layer for ceramic matrix composite substrate |
| CN114807723B (en) * | 2022-04-13 | 2023-01-17 | 北京科技大学 | Metal ceramic composite coating and preparation method thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3309897B2 (en) * | 1995-11-15 | 2002-07-29 | 住友電気工業株式会社 | Ultra-hard composite member and method of manufacturing the same |
| JP3522588B2 (en) * | 1999-05-26 | 2004-04-26 | トーカロ株式会社 | Chromium carbide cermet sprayed coating member excellent in high-temperature hardness and method for producing the same |
| ITRM20030602A1 (en) * | 2003-12-24 | 2005-06-25 | Ct Sviluppo Materiali Spa | MULTILAYER COATING PRODUCTION PROCEDURE |
| US7635515B1 (en) | 2004-04-08 | 2009-12-22 | Powdermet, Inc | Heterogeneous composite bodies with isolated lenticular shaped cermet regions |
| JP5013364B2 (en) | 2006-09-12 | 2012-08-29 | 独立行政法人物質・材料研究機構 | Cermet film forming method and cermet coating member obtained thereby |
-
2010
- 2010-02-03 BR BRPI1005423A patent/BRPI1005423A2/en not_active IP Right Cessation
- 2010-02-03 SG SG2011055803A patent/SG173515A1/en unknown
- 2010-02-03 US US12/699,779 patent/US8460796B2/en active Active
- 2010-02-03 CA CA2751250A patent/CA2751250C/en active Active
- 2010-02-03 WO PCT/US2010/023097 patent/WO2010123612A2/en active Application Filing
- 2010-02-03 EP EP10767468A patent/EP2393954A2/en not_active Withdrawn
- 2010-02-03 CN CN2010800122672A patent/CN102356175A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109844177A (en) * | 2016-08-16 | 2019-06-04 | 塞拉姆涂料股份有限公司 | The thermal spraying of ceramic material |
| CN109844177B (en) * | 2016-08-16 | 2022-05-17 | 塞拉姆涂料股份有限公司 | Thermal spraying of ceramic materials |
| CN111148567A (en) * | 2017-10-13 | 2020-05-12 | Sabic环球技术有限责任公司 | Process for producing an elastomer agglomerate composition, elastomer agglomerate composition and use thereof |
| CN111148567B (en) * | 2017-10-13 | 2022-04-15 | Sabic环球技术有限责任公司 | Process for producing an elastomer agglomerate composition, elastomer agglomerate composition and use thereof |
| CN109177367A (en) * | 2018-09-07 | 2019-01-11 | 昆明理工大学 | A kind of discontinuous stratiform structural composite material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CA2751250A1 (en) | 2010-10-28 |
| SG173515A1 (en) | 2011-09-29 |
| CA2751250C (en) | 2017-04-25 |
| BRPI1005423A2 (en) | 2018-04-10 |
| US8460796B2 (en) | 2013-06-11 |
| EP2393954A2 (en) | 2011-12-14 |
| WO2010123612A2 (en) | 2010-10-28 |
| WO2010123612A3 (en) | 2011-04-07 |
| US20100203255A1 (en) | 2010-08-12 |
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